CN113259816A - Vibrating diaphragm and preparation method and application thereof - Google Patents
Vibrating diaphragm and preparation method and application thereof Download PDFInfo
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- 238000000034 method Methods 0.000 claims abstract description 25
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- 150000004706 metal oxides Chemical class 0.000 claims abstract description 18
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- 239000002585 base Substances 0.000 claims description 34
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- 239000002243 precursor Substances 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 27
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- 238000001723 curing Methods 0.000 claims description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 13
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- 238000000576 coating method Methods 0.000 claims description 13
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- 230000032683 aging Effects 0.000 claims description 10
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 9
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- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 5
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims description 5
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- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 4
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
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- 239000004408 titanium dioxide Substances 0.000 description 2
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 description 2
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- GSWGDDYIUCWADU-UHFFFAOYSA-N aluminum magnesium oxygen(2-) Chemical compound [O--].[Mg++].[Al+3] GSWGDDYIUCWADU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 229910003472 fullerene Inorganic materials 0.000 description 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R7/00—Diaphragms for electromechanical transducers; Cones
- H04R7/02—Diaphragms for electromechanical transducers; Cones characterised by the construction
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R31/00—Apparatus or processes specially adapted for the manufacture of transducers or diaphragms therefor
- H04R31/003—Apparatus or processes specially adapted for the manufacture of transducers or diaphragms therefor for diaphragms or their outer suspension
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R2307/00—Details of diaphragms or cones for electromechanical transducers, their suspension or their manufacture covered by H04R7/00 or H04R31/003, not provided for in any of its subgroups
- H04R2307/023—Diaphragms comprising ceramic-like materials, e.g. pure ceramic, glass, boride, nitride, carbide, mica and carbon materials
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R2307/00—Details of diaphragms or cones for electromechanical transducers, their suspension or their manufacture covered by H04R7/00 or H04R31/003, not provided for in any of its subgroups
- H04R2307/027—Diaphragms comprising metallic materials
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Signal Processing (AREA)
- Multimedia (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a vibrating diaphragm and a preparation method and application thereof, wherein the vibrating diaphragm comprises a base layer and metal oxide ceramic layers arranged on two sides of the base layer; the thickness of the diaphragm is 45-55 μm; the thickness of the metal oxide ceramic layers on the two sides is 5-10 mu m. The vibrating diaphragm is not provided with the glue layer, so that additional anti-corrosion surface treatment is not needed, the process flow of the vibrating diaphragm is reduced, the product yield is increased, the vibrating diaphragm is more resistant to environmental corrosion, and the damping performance is better.
Description
Technical Field
The invention relates to the technical field of diaphragms, in particular to a diaphragm and a preparation method and application thereof.
Background
The diaphragm is one of the main parts of the loudspeaker, and the main structure of the existing ceramic diaphragm is a ceramic layer, an adhesion layer or a substrate layer.
CN202679596U discloses a well, high pitch loudspeaker ceramic diaphragm structure, belong to the stereo set class, ceramic diaphragm includes the raw materials layer that plural ceramic powder layer and plural number and these some ceramic powder layers mix and form the anchor coat, this anchor coat mixes with plural glue layer again and forms an extremely thin ceramic substrate layer, pass through moulding-die forming with this ceramic substrate layer and make this ceramic substrate layer form a half-circular arc vibrating diaphragm, the frequency response of the hard and more frivolous ceramic structure physical characteristic promotion loudspeaker of intensity by this, and make loudspeaker can make good in the clear broadcast of former sound, high tone quality, the event is suitable for and uses the vibrating diaphragm in, on the high pitch loudspeaker. However, the ceramic layer is mainly made of alumina, zirconia, silica and the like, the adhesion layer contains acrylic acid, epoxy and the like, the base material is conventional membrane, metal or ceramic, and the adhesion layer is mainly made of adhesive, so that the adhesion layer is easy to crack due to temperature resistance and self-adhesive property after curing, and the diaphragm is ineffective. Meanwhile, because of multilayer molding, ceramic needs to be sintered firstly for hot pressing, the processing flow is complex, the control parameters are more, and the large-scale production is not facilitated, and the pure ceramic diaphragm is mainly zirconium ceramic, magnesium aluminum oxide ceramic and the like, and has larger structural pores, lower ductility and easy cracking.
CN105323697A discloses a method for manufacturing a composite diaphragm and a diaphragm manufactured by using the method, wherein the surface of the disclosed diaphragm is coated with a reinforcing material, and the reinforcing material is made of any one of alumina, silica, zirconia, titanium dioxide, calcium phosphate, aluminum hydroxide, zinc oxide, silicon carbide, fullerene, carbon nanotube and graphene, or a mixture of the above materials; the disclosed manufacturing method comprises the following steps: and mixing the reinforcing material with the hot melt adhesive, heating and curing to finish the preparation of the composite diaphragm. The preparation method of the vibrating diaphragm disclosed by the invention is to mix the reinforcing materials such as zirconia or titanium dioxide and the like with the hot melt adhesive and then heat and solidify the reinforcing materials, and the preparation process is relatively complex.
In conclusion, it is important to develop a diaphragm with simple process, environmental corrosion resistance and better damping performance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the vibrating diaphragm, and the preparation method and the application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a diaphragm, including a base layer and metal oxide ceramic layers disposed on two sides of the base layer;
the thickness of the diaphragm is 45-55 μm, such as 46 μm, 47 μm, 48 μm, 49 μm, 50 μm, 51 μm, 52 μm, 53 μm, 54 μm, and the like;
the thickness of the metal oxide ceramic layers on both sides is 5 to 10 μm, for example, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm, 8 μm, 8.5 μm, 9 μm, 9.5 μm, etc. independently.
At present, the metal ball top vibrating diaphragm and the like are usually formed by punching aluminum and titanium sheets, and are subjected to external spraying or anodic oxidation treatment, so that the biggest problem of the metal vibrating diaphragm is that the internal loss is small, and the peak-valley value of the frequency response in a high frequency band is large. In the continuous vibration of the loudspeaker, the non-effective vibration rebound is reduced, the instantaneous response is improved, the fluctuation range of the peak-valley value can be reduced, the frequency response curve is smoothed, and the frequency of the frequency response is prolonged in a high frequency band. The vibrating diaphragm is simple in composition and avoids the influence of the glue layer on the vibrating diaphragm; on the basis of the advantages of the traditional metal ball top vibrating diaphragm, the metal oxide ceramic layer does not need additional anti-corrosion surface treatment relative to the traditional metal layer, so that the process flow of the vibrating diaphragm is reduced, the product yield is increased, the vibrating diaphragm is more resistant to environmental corrosion, and the damping performance is better; in addition, the thickness of the whole vibrating diaphragm and the thickness of the ceramic layer are adjusted, so that the comprehensive performance of the vibrating diaphragm is more excellent.
Preferably, the material of the base layer includes a simple metal and/or an alloy.
Preferably, the elemental metal comprises aluminum and/or titanium.
Preferably, the metal oxide comprises titanium oxide and/or aluminum oxide.
In a second aspect, the present invention provides a method for preparing a diaphragm according to the first aspect, where the method includes the following steps: preparing raw materials of the ceramic layer into gel by a sol-gel method, coating the gel on a base layer, and then sequentially drying, curing and calcining to form the metal oxide ceramic layer, thereby obtaining the vibrating diaphragm.
The ceramic layer is prepared by coating raw materials through a sol-gel method and then calcined, so that metal oxides are directly deposited on the base layer, the formed vibrating diaphragm has better flexibility, and the problem that the vibrating diaphragm is cracked due to extrusion and collision in the processes of processing, detection, packaging and transportation can be effectively solved.
Preferably, the shape of the base layer comprises a dome or a cone.
The spherical top and the conical top are respectively a spherical top vibrating diaphragm in a segment shape or a conical cone vibrating diaphragm.
Preferably, the coating further comprises pretreating the base layer.
Preferably, the pretreatment comprises in sequence: alkali washing, first water washing, ultrasonic treatment, second water washing and drying.
Preferably, the time of the alkaline washing is 10-15min, such as 11min, 12min, 13min, 14min and the like.
Preferably, the time of the ultrasound is 10-15min, such as 11min, 12min, 13min, 14min, and the like.
Preferably, the solvent of the ultrasound comprises ethanol and/or acetone.
Preferably, the sol-gel process comprises the steps of:
(1) preparing a precursor solvent A: mixing 10-50 parts by weight (e.g., 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, 35 parts by weight, 40 parts by weight, 45 parts by weight, etc.) of a ceramic layer preparation raw material, 10-40 parts by weight (e.g., 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, 35 parts by weight, etc.) of a first solvent and 100-200 parts by weight (e.g., 120 parts by weight, 140 parts by weight, 160 parts by weight, 180 parts by weight, etc.) of a second solvent to obtain the precursor solvent A;
(2) preparing a solution C: mixing the precursor solvent A, 5-60 parts by weight (e.g., 10 parts by weight, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, 35 parts by weight, 40 parts by weight, 45 parts by weight, 50 parts by weight, 55 parts by weight, etc.) of the solvent B and a pH regulator to obtain a solution C;
(3) aging the solution C to obtain gel;
(4) coating the gel on the surface of a base layer, and then sequentially drying and curing;
(5) and (4) after the steps (1) to (4) are carried out at least once, calcining to form a ceramic layer, and obtaining the vibrating diaphragm.
According to the invention, when the steps (1) to (4) are repeated, all the used preparation raw materials and process parameters can be adaptively adjusted, and are not required to be completely the same.
Preferably, the step (1) specifically comprises: preparing a precursor solvent A: 10-50 parts by weight (for example, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, 35 parts by weight, 40 parts by weight, 45 parts by weight, etc.) of a ceramic layer preparation raw material and 10-40 parts by weight (for example, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, 35 parts by weight, etc.) of a first solvent are stirred and mixed for the first time, and then the mixed solution is stirred and mixed for the second time with 100 parts by weight (for example, 120 parts by weight, 140 parts by weight, 160 parts by weight, 180 parts by weight, etc.) of a second solvent to obtain the precursor solvent A.
Preferably, the time for the first stirring and mixing is 10-30min, such as 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min, etc.
Preferably, the time for the second stirring and mixing is 60-120min, such as 65min, 70min, 75min, 80min, 85min, 90min, 95min, 100min, 105min, 110min, 115min, and the like.
Preferably, the ceramic layer preparation raw material comprises any one of tetrabutyl titanate, n-butyl titanate, tetraisopropyl titanate, aluminum chloride hexahydrate, aluminum nitrate nonahydrate, aluminum isopropoxide or aluminum tri-sec-butoxide or a combination of at least two of them, wherein a typical but non-limiting combination comprises: combinations of tetrabutyl titanate, n-butyl titanate, and tetraisopropyl titanate, combinations of aluminum chloride hexahydrate, aluminum nitrate nonahydrate, aluminum isopropoxide, and aluminum tri-sec-butoxide, combinations of tetraisopropyl titanate, aluminum chloride hexahydrate, and aluminum nitrate nonahydrate, and the like.
Preferably, the first solvent comprises any one of or a combination of at least two of diethanolamine, acetone, or polyethylene glycol, wherein typical but non-limiting combinations include: combinations of diethanolamine and acetone, combinations of acetone and polyethylene glycol, combinations of diethanolamine, acetone and polyethylene glycol, and the like.
Preferably, the second solvent comprises any one of, or a combination of at least two of, polyvinyl alcohol, ethanol, propanol, or acetone, where typical but non-limiting combinations include: combinations of polyvinyl alcohol and ethanol, combinations of ethanol, propanol, and acetone, combinations of polyvinyl alcohol, ethanol, propanol, and acetone, and the like.
Preferably, the aging time in step (3) is 2-24h, such as 4h, 6h, 8h, 10h, 15h, 14h, 16h, 18h, 20h, 22h, etc.
Preferably, the temperature of the curing in step (4) is 70-90 ℃, such as 72 ℃, 74 ℃, 76 ℃, 78 ℃, 80 ℃, 82 ℃, 84 ℃, 86 ℃, 88 ℃ and the like.
Preferably, the curing time is 1-3h, such as 1.2h, 1.4h, 1.6h, 1.8h, 2h, 2.2h, 2.4h, 2.6h, 2.8h, and the like.
Preferably, the temperature of the calcination in step (5) is 450-.
Preferably, the calcination is carried out for a time of 12 to 24h, such as 14h, 16h, 18h, 20h, 22h, etc.
As a preferred technical scheme, the preparation method comprises the following steps:
(1') subjecting the base layer to the following pretreatment in order: alkali washing for 10-15min, first water washing, ultrasonic washing in ethanol and/or acetone for 10-15min, second water washing and drying;
(2') preparing a precursor solvent A: stirring and mixing 10-50 parts by weight of ceramic layer preparation raw materials and 10-40 parts by weight of first solvent for 10-30min for the first time, and stirring and mixing the mixed solution and 100-200 parts by weight of second solvent for the second time for 60-120min to obtain a precursor solvent A;
(3') preparation of solution C: mixing a precursor solvent A, 5-60 parts by weight of a solvent B and a pH regulator to obtain a solution C;
(4') ageing the solution C for 2-24h to obtain gel;
(5') coating the gel on the surface of the base layer, drying and curing for 1-3h at 70-90 ℃;
(6') after the steps (2') - (5') are carried out at least once, calcining at 450 ℃ and 500 ℃ for 12-24h to form a ceramic layer, thus obtaining the diaphragm.
In a third aspect, the present invention provides a loudspeaker comprising the diaphragm of the first aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) the processing is convenient, only sintering treatment is needed after coating, gluing is not needed between metal and ceramic, additional anti-corrosion surface treatment is not needed, the process flow of the vibrating diaphragm is reduced, and the product yield is increased. The ceramic layers are all metal oxide components, so that the ceramic layers are more resistant to environmental corrosion and more excellent in weather resistance;
(2) the loss factor is more than 0.054, and the damping performance is excellent;
(3) young's modulus of 95GPa or more and density of 3.24g/cm3The specific modulus is 31.48X 106m2/s2The density is small, the specific modulus is high, an excellent acoustic curve can be achieved in the ultrahigh frequency field of more than 25-30k, and the tone quality is clear and thorough;
(4) the flexibility is better, the elongation after fracture is more than 12.1 percent, and the vibration diaphragm can be effectively prevented from being cracked due to extrusion and collision in the processes of processing, detection, packaging and transportation;
(5) the waterproof performance and the cyclic thermal shock performance are excellent, 30 cyclic thermal shock vibrating diaphragms do not fall off, and the industrial standard is met in the Baige test.
Drawings
Fig. 1 is a schematic view of a diaphragm according to embodiment 1;
FIG. 2 is a schematic view of a diaphragm according to embodiment 3;
wherein, 1-a base layer; 21-a first ceramic layer; 22-a second ceramic layer; 31-a third ceramic layer; 32-fourth ceramic layer.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The present embodiment provides a diaphragm, as shown in fig. 1, the diaphragm includes a base layer 1 (an aluminum sheet), and a first ceramic layer 21 (titanium oxide, thickness is 5 μm) and a second ceramic layer 22 (titanium oxide, thickness is 5 μm) disposed on two sides of the base layer, and the thickness of the diaphragm is 45 μm.
The preparation method of the diaphragm comprises the following steps:
(1) stamping the base layer with the thickness of 35 mu m into a spherical top shape on a die, and sequentially carrying out the following pretreatment on the stamped base layer: removing oil by alkali washing for 10min, washing with water for the first time, performing ultrasonic treatment in ethanol for 10min, washing with water for the second time, and drying at 50 ℃;
(2) preparing a precursor solvent A: stirring and mixing 30 parts by weight of a ceramic layer preparation raw material (tetrabutyl titanate) and 20 parts by weight of a first solvent (10 parts of diethanolamine and 10 parts of acetone) for 10min for the first time, and stirring and mixing the mixed solution and 100 parts by weight of a second solvent (ethanol) for the second time for 60min to obtain a precursor solvent A;
(3) preparing a solvent B: mixing 25 parts by weight of a solvent (20 parts by weight of ethanol and 5 parts by weight of deionized water) and a pH regulator (nitric acid), regulating the pH value to 3, and stirring for 30min at 30 ℃ by using a magnetic stirrer to obtain a solvent B;
(4) dripping the solvent B into the precursor solvent A, violently stirring for 30min, mixing to obtain a solution C, and aging for 16h to obtain gel;
(5) and fixing the base layer at a spin coating center through a central vacuum suction device of a spin coater at the rotating speed of 300r/min, spin-coating, drying, curing at 70 ℃ for 1h, and calcining at 450 ℃ for 12h to form a ceramic layer, thus obtaining the diaphragm.
Example 2
This embodiment provides a vibrating diaphragm, the vibrating diaphragm include basic unit (aluminum sheet) and set up in the metal oxide (aluminium oxide) ceramic layer of basic unit both sides, the thickness of vibrating diaphragm is 45 μm, the thickness of the metal oxide ceramic layer of both sides is 5 μm.
The preparation method of the diaphragm comprises the following steps:
(1) stamping the base layer with the thickness of 35 mu m into a spherical top shape on a die, and sequentially carrying out the following pretreatment on the stamped base layer: removing oil by alkali washing for 15min, washing with water for the first time, performing ultrasonic treatment in ethanol for 15min, washing with water for the second time, and drying at 50 ℃;
(2) preparing a precursor solvent A: 60 parts by weight of ceramic layer preparation raw materials (aluminum chloride hexahydrate and aluminum nitrate nonahydrate in a mass ratio of 1:1) and 20 parts by weight of first solvent (diethanolamine and polyethylene glycol in a mass ratio of 1: 3) are stirred and mixed for the first time for 30min, and then the mixed solution and 200 parts by weight of second solvent (propanol) are stirred and mixed for the second time for 120min to obtain a precursor solvent A;
(3) preparing a solvent B: adding 20 parts of a mixture of ammonia water with the pH value of 12, a sodium bicarbonate solution and a sodium carbonate solution (the mass ratio of the ammonia water to the sodium bicarbonate solution to the sodium carbonate solution is 1:1:1) into the precursor solvent A, rapidly stirring for 60min at normal temperature by using a magnetic stirrer to obtain a solvent B, and filtering the precipitate in the solution B by using a suction filter;
(4) preparing a solution C: heating solvent B in water bath at 60 deg.C for 60min to obtain white flocculent solution, adding 10 weight parts of pH regulator (hydrochloric acid) with pH value of 3 dropwise into the solution, peptizing, stirring thoroughly, mixing, and aging for 10 h;
(5) and fixing the base layer at a spin coating center through a central vacuum suction device of a spin coater at the rotating speed of 800r/min, spin-coating, drying, curing at 90 ℃ for 3h, and calcining at 500 ℃ for 24h to form a ceramic layer, thus obtaining the diaphragm.
Example 3
The present embodiment provides a diaphragm, as shown in fig. 2, the diaphragm includes a third ceramic layer 31 (titanium oxide, with a thickness of 2.5 μm), a first ceramic layer 21 (aluminum oxide, with a thickness of 1.5 μm), a base layer 1 (aluminum alloy, available from shin electro-acoustic technologies ltd., incorporated by reference), a second ceramic layer 22 (aluminum oxide, with a thickness of 2 μm), and a fourth ceramic layer 32 (titanium oxide, with a thickness of 2 μm), which are stacked in this order, and the thickness of the diaphragm is 48 μm.
The preparation method of the diaphragm comprises the following steps:
(1) stamping the base layer with the thickness of 40 mu m into a spherical top shape on a die, and sequentially carrying out the following pretreatment on the stamped base layer: removing oil with alkali for 12min, washing with water for the first time, performing ultrasonic treatment in ethanol for 13min, washing with water for the second time, and drying at 50 deg.C;
(2) preparing a precursor solvent A: stirring and mixing 15 parts by weight of ceramic layer preparation raw material (aluminum isopropoxide) and 15 parts by weight of first solvent (15 parts by weight of diethanolamine) for the first time for 20min, and stirring and mixing the mixed solution and 150 parts by weight of second solvent (polyethylene glycol and ethanol in a mass ratio of 1: 10) for the second time for 100min to obtain a precursor solvent A;
(3) preparing a solvent B: adding 15 parts of ammonia water with the pH value of 10 into the precursor solvent A, quickly stirring for 50min at normal temperature by using a magnetic stirrer to obtain a solvent B, and filtering the precipitate in the solution B by using a suction filter;
(4) preparing a solution C: heating the solvent B in water bath at 50 ℃ for 40min to obtain white flocculent solution, dropwise adding 10 parts by weight of pH regulator (nitric acid) with the pH value of 1 into the solution, peptizing, fully stirring and mixing, and aging for 8 h;
(5) fixing the base layer at a spin coating center through a central vacuum suction device of a spin coater at a rotation speed of 800r/min, spin-coating, drying, and curing at 80 ℃ for 2 h;
(6) preparing a precursor solvent A': 50 parts by weight of ceramic layer preparation raw materials (namely n-butyl titanate and tetraisopropyl titanate with the mass ratio of 1:1) and 40 parts by weight of first solvent (20 parts of diethanolamine and 20 parts of acetone) are stirred and mixed for the first time for 25min, and then the mixed solution and 200 parts by weight of second solvent (ethanol) are stirred and mixed for the second time for 75min to obtain a precursor solvent A';
(7) preparing a solvent B': mixing 50 parts by weight of a solvent (40 parts by weight of ethanol and 10 parts by weight of deionized water) and a pH regulator (concentrated sulfuric acid), adjusting the pH value to 3, and stirring for 50min at 50 ℃ by using a magnetic stirrer to obtain a solvent B';
(8) dripping the solvent B ' into the precursor solvent A ', vigorously stirring for 40min, and mixing to obtain a solution C ', and aging for 24h to obtain gel;
(9) and fixing the base layer in a spin coating center through a central vacuum suction device of a spin coater at the rotating speed of 700r/min, spin-coating, drying, curing at 60 ℃ for 2.5h, and calcining at 480 ℃ for 36h to form a ceramic layer, thus obtaining the diaphragm.
Example 4
Example 4 is different from example 1 in that the metal oxide ceramic layers on both sides have a thickness of 10 μm, and the rest is the same as example 1.
Comparative examples 1 to 2
Comparative examples 1-2 are different from example 1 in that the thicknesses of the metal oxide ceramic layers on both sides are 2 μm and 12 μm, and the rest is the same as example 1.
Comparative example 3
This embodiment provides a vibrating diaphragm, the vibrating diaphragm includes the first ceramic layer (titanium oxide, and thickness is 5 μm), first glue film (thickness is 2 μm), basic unit (aluminum sheet), second glue film (thickness is 2 μm) and the second ceramic layer (titanium oxide, and thickness is 5 μm) that stack gradually the setting, the thickness of vibrating diaphragm is about 45 μm.
The preparation method of the diaphragm comprises the following steps:
(1) carrying out alkali washing and oil removal on the aluminum substrate, ultrasonically removing residual impurities and a tiny oil film in ethanol, and heating and drying;
(2) coating adhesive layers on two sides of a base material by using a coating machine, wherein the adhesive layers are hydroxyethyl methacrylate (purchased from Lizechangsheng source science and technology Co., Ltd.), the thickness of the adhesive layers is 2 mu m, and heating is carried out at 70 ℃ until the adhesive layers are primarily cured;
(3) spraying titanium oxide slurry on the adhesive layer, and curing and sintering at 450 ℃ until the thickness of the single-side ceramic layer reaches 5 mu m;
(4) and putting the sintered material plate into a die to be punched into a flat plate or to be molded by pressing.
Performance testing
Examples 1-4 and comparative examples 1-3 were tested as follows:
(1) young's modulus: testing was carried out according to the method disclosed in ASTM-D882;
(2) density: testing by adopting a density tester with the model of MAY-Entris 120;
(3) waterproof grade: testing according to a method disclosed in national standard GB 4208-;
(4) and (3) testing the grids: the test is carried out according to the method disclosed by the national standard GB/T9286-1998 test for marking the color paint, the varnish and the paint film;
(5) cyclic thermal shock: testing is carried out according to the method disclosed in the national standard GB/T3298-;
(6) elongation at break: testing according to the national standard GB228-2000 GBT 228-;
(7) damping performance: testing by using a KLIPPLE sound field signal tester with a damping module;
(8) specific modulus: and (3) carrying out division calculation on the Young modulus measured by the method in (1) and the density measured by the method in (2).
The test results are summarized in tables 1 and 2.
TABLE 1
TABLE 2
As can be seen from the analysis of the data in tables 1 and 2, the diaphragm of the present invention has the following advantages:
(1) the processing is convenient, only sintering treatment is needed after coating, gluing is not needed between metal and ceramic, additional anti-corrosion surface treatment is not needed, the process flow of the vibrating diaphragm is reduced, and the product yield is increased. The ceramic layers are all metal oxide components, so that the ceramic layers are more resistant to environmental corrosion and more excellent in weather resistance;
(2) the loss factor is more than 0.054, and the damping performance is excellent;
(3) young's modulus of 95GPa or more and density of 3.24g/cm3The specific modulus is 31.48X 106m2/s2The density is small, the specific modulus is high, an excellent acoustic curve can be achieved in the ultrahigh frequency field of more than 25-30k, and the tone quality is clear and thorough;
(4) the flexibility is better, the elongation after fracture is more than 12.1 percent, and the vibration diaphragm can be effectively prevented from being cracked due to extrusion and collision in the processes of processing, detection, packaging and transportation;
(5) the waterproof performance and the cyclic thermal shock performance are excellent, 30 cyclic thermal shock vibrating diaphragms do not fall off, and the industrial standard is met in the Baige test.
As can be seen from the analysis of examples 1 and 4 and comparative examples 1 to 2, comparative examples 1 to 2 are inferior to example 1 in performance, and it was confirmed that the diaphragm obtained with the ceramic layer having a thickness in the range of 5 to 10 μm is superior in overall performance.
As can be seen from the analysis of comparative example 3 and example 1, the performance of comparative example 3 is inferior to that of example 1, and the sol-gel method for preparing the ceramic layer of the diaphragm is proved to have better comprehensive performance.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The vibrating diaphragm is characterized by comprising a base layer and metal oxide ceramic layers arranged on two sides of the base layer;
the thickness of the diaphragm is 45-55 μm;
the thicknesses of the metal oxide ceramic layers on the two sides are respectively 5-10 mu m.
2. The diaphragm of claim 1, wherein the base layer is made of a metal simple substance and/or an alloy;
preferably, the elemental metal comprises aluminum and/or titanium.
3. The diaphragm of claim 1 or 2, wherein the metal oxide comprises titanium oxide and/or aluminum oxide.
4. A method of manufacturing a diaphragm according to any one of claims 1 to 3, comprising the steps of: preparing raw materials of the ceramic layer into gel by a sol-gel method, coating the gel on a base layer, and then sequentially drying, curing and calcining to form the metal oxide ceramic layer, thereby obtaining the vibrating diaphragm.
5. The method of claim 4, wherein the shape of the base layer comprises a spherical apex or a conical apex;
preferably, the coating also comprises the step of pretreating the base layer;
preferably, the pretreatment comprises in sequence: alkali washing, first water washing, ultrasonic treatment, second water washing and drying;
preferably, the time of the alkali washing is 10-15 min;
preferably, the time of the ultrasonic treatment is 10-15 min;
preferably, the solvent of the ultrasound comprises ethanol and/or acetone.
6. The method according to claim 4 or 5, wherein the sol-gel process comprises the steps of:
(1) preparing a precursor solvent A: mixing 10-50 parts by weight of ceramic layer preparation raw material, 10-40 parts by weight of first solvent and 100-200 parts by weight of second solvent to obtain precursor solvent A;
(2) preparing a solution C: mixing a precursor solvent A, 5-60 parts by weight of a solvent B and a pH regulator to obtain a solution C;
(3) aging the solution C to obtain gel;
(4) coating the gel on the surface of a base layer, and then sequentially drying and curing;
(5) and (4) after the steps (1) to (4) are carried out at least once, calcining to form a ceramic layer, and obtaining the vibrating diaphragm.
7. The preparation method according to claim 6, wherein the step (1) specifically comprises: preparing a precursor solvent A: stirring and mixing 10-50 parts by weight of ceramic layer preparation raw materials and 10-40 parts by weight of first solvent for the first time, and stirring and mixing the mixed solution and 100-200 parts by weight of second solvent for the second time to obtain a precursor solvent A;
preferably, the time for the first stirring and mixing is 10-30 min;
preferably, the time for stirring and mixing for the second time is 60-120 min;
preferably, the ceramic layer preparation raw material comprises any one or a combination of at least two of tetrabutyl titanate, n-butyl titanate, tetraisopropyl titanate, aluminum chloride hexahydrate, aluminum nitrate nonahydrate, aluminum isopropoxide or aluminum tri-sec-butyl alkoxide;
preferably, the first solvent comprises any one of or a combination of at least two of diethanolamine, acetone, or polyethylene glycol;
preferably, the second solvent comprises any one of polyvinyl alcohol, ethanol, propanol or acetone or a combination of at least two thereof.
8. The method according to claim 6, wherein the aging time in the step (3) is 2 to 24 hours;
preferably, the temperature of the curing in the step (4) is 70-90 ℃;
preferably, the curing time is 1-3 h;
preferably, the temperature of the calcination in step (5) is 450-500 ℃;
preferably, the calcination time is 12-24 h.
9. The method according to any one of claims 4 to 8, characterized by comprising the steps of:
(1') subjecting the base layer to the following pretreatment in order: alkali washing for 10-15min, first water washing, ultrasonic washing in ethanol and/or acetone for 10-15min, second water washing and drying;
(2') preparing a precursor solvent A: stirring and mixing 10-50 parts by weight of ceramic layer preparation raw materials and 10-40 parts by weight of first solvent for 10-30min for the first time, and stirring and mixing the mixed solution and 100-200 parts by weight of second solvent for the second time for 60-120min to obtain a precursor solvent A;
(3') preparation of solution C: mixing a precursor solvent A, 5-60 parts by weight of a solvent B and a pH regulator to obtain a solution C;
(4') ageing the solution C for 2-24h to obtain gel;
(5') coating the gel on the surface of the base layer, drying and curing for 1-3h at 70-90 ℃;
(6') after the steps (2') - (5') are carried out at least once, calcining at 450 ℃ and 500 ℃ for 12-24h to form a ceramic layer, thus obtaining the diaphragm.
10. A loudspeaker, characterized in that the loudspeaker comprises a diaphragm according to any one of claims 1 to 3.
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| US6327372B1 (en) * | 1999-01-05 | 2001-12-04 | Harman International Industries Incorporated | Ceramic metal matrix diaphragm for loudspeakers |
| WO2006120387A2 (en) * | 2005-05-11 | 2006-11-16 | Sheffield Hallam University | Sol-gel derived coating |
| US20070098905A1 (en) * | 2004-06-17 | 2007-05-03 | Electricite De France Service National | Method for preparing metal oxide layers |
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| CN201758445U (en) * | 2010-07-23 | 2011-03-09 | 东莞市阳证电器配件有限公司 | Metal loudspeaker vibration diaphragm coated with ceramic layer |
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| CN108337622A (en) * | 2018-03-05 | 2018-07-27 | 苏州市艾倍力精密电子有限公司 | A kind of acoustic diaphragm, diaphragm materials and vibrating diaphragm preparation process |
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2021
- 2021-05-28 CN CN202110590497.7A patent/CN113259816A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6327372B1 (en) * | 1999-01-05 | 2001-12-04 | Harman International Industries Incorporated | Ceramic metal matrix diaphragm for loudspeakers |
| US20070098905A1 (en) * | 2004-06-17 | 2007-05-03 | Electricite De France Service National | Method for preparing metal oxide layers |
| US20080286590A1 (en) * | 2004-08-24 | 2008-11-20 | Albright & Wilson (Australia) Limited | Ceramic and Metallic Components and Methods for Their Production from Flexible Gelled Materials |
| WO2006120387A2 (en) * | 2005-05-11 | 2006-11-16 | Sheffield Hallam University | Sol-gel derived coating |
| CN201758445U (en) * | 2010-07-23 | 2011-03-09 | 东莞市阳证电器配件有限公司 | Metal loudspeaker vibration diaphragm coated with ceramic layer |
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